CN112745638B - High-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material and preparation method thereof - Google Patents
High-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention discloses a high-voltage resistant m-ABA-SiO2The alicyclic epoxy resin nano composite insulating material is prepared from SiO2After the nano particles are grafted with the voltage stabilizer m-aminobenzoic acid, the nano particles are introduced into the alicyclic epoxy resin matrix. In the nano composite insulating material of the invention, SiO is used2The interface action of the nano particles and the alicyclic epoxy resin traps a part of charges, and the m-aminobenzoic acid captures a part of high-energy electrons, so that the charge distribution condition of a matrix under a certain voltage is improved, and the voltage breakdown resistance is improved.
Description
Technical Field
The invention relates to high-voltage-resistant m-ABA-SiO2A/alicyclic epoxy resin nano composite insulating material and a preparation method thereof belong to the field of insulation and high voltage resistance.
Background
The increase of energy demand, the uneven energy distribution, the intensification of urban construction need to develop superhigh pressure, large capacity power equipment and high voltage power electronic equipment, and these novel power equipment face complicated insulating demand. In fact, a sufficiently high electric field will enable electrons inside the insulating material to tunnel from the valence band to the conduction band. These electrons are accelerated by an electric field to collide with other atoms, and then ionized electrons are generated by secondary collision. Electrical breakdown occurs completely after the total amount of free electrons exceeds a threshold, and such electrical breakdown is catastrophic to the electrical device. The alicyclic epoxy resin does not contain aromatic unsaturated rings, has high voltage and electric leakage resistance, high heat resistance, excellent bonding performance with a core rod interface and simple preparation process, and is an ideal insulating material with excellent performance. The alicyclic epoxy resin does not lack electrons in the structure, and the attack of amine nucleophiles is difficult, so that the use of amine curing agents with high toxicity and strong volatility can be avoided, and the alicyclic epoxy resin is environment-friendly to human bodies. However, in the synthesis process of the resin, some chemical defects or physical impurities are always introduced, and a tiny current passes through the matrix under the action of voltage, so that how to reduce the passage of the current is important for improving the high-voltage resistance of the alicyclic epoxy resin.
The commonly used methods for improving the insulating property of the matrix at present are as follows: 1. blending different polymers; 2. by adding the nano composite insulating material, the nano particles can introduce deep defects into the matrix and trap charges in the traps; 3. and adding a voltage stabilizer, such as a benzene ring compound, wherein a conjugated structure contained in the voltage stabilizer can capture high-energy electrons. The research of the invention finds that: the nano silicon dioxide is a three-dimensional net structure, has good compatibility with an alicyclic epoxy resin matrix, but has high surface activity and is easy to agglomerate. The voltage stabilizer is grafted on the nano silicon dioxide, so that the agglomeration of the nano silicon dioxide can be avoided on one hand, and the migration of the small molecular voltage stabilizer m-aminobenzoic acid in a matrix can be avoided on the other hand, thereby leading the nano SiO particles to be2And the voltage stabilizer plays a synergistic role in the alicyclic epoxy resin.
Disclosure of Invention
The invention provides a high-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material and preparation method thereof, aiming at introducing voltage stabilizer grafted SiO2The nanoparticle particles improve the electrical breakdown resistance of the material.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the invention firstly discloses a voltage stabilizer grafted SiO2Nanoparticles, characterized by: is in SiO2The nano particles are grafted with a voltage stabilizer m-aminobenzoic acid which is marked as m-ABA-SiO2And (3) nanoparticles.
The voltage stabilizer grafted SiO of the invention2The preparation method of the nano-particles comprises the following steps:
The invention also discloses high-voltage-resistant m-ABA-SiO2The alicyclic epoxy resin nano composite insulating material is characterized in that: the nano composite insulating material is prepared by adding m-ABA-SiO described in claim 1 into alicyclic epoxy resin matrix2And (3) nanoparticles.
Preferably, m-ABA-SiO in the nano composite insulating material2The mass percentage of the nano particles is 1-5%.
The high-voltage-resistant m-ABA-SiO2The preparation method of the alicyclic epoxy resin nano composite insulating material comprises the following steps:
firstly, adding liquid alicyclic epoxy resin, anhydride curing agent and accelerator DMP-30 into a beaker, and fully stirring at room temperature to obtain a transparent solution;
then m-ABA is added into the transparent solution under the condition of rapid stirring-SiO2Continuously stirring the nano particles until the solution is clear, and then ultrasonically dispersing the nano particles uniformly (so that bubbles in the solution are broken, and nano particles are prevented from agglomerating) to obtain a mixed solution;
finally, curing the mixed solution to obtain the high-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material.
Preferably, the mass ratio of the liquid alicyclic epoxy resin, the anhydride curing agent and the accelerator DMP-30 is 100:120: 5.
Preferably, the curing conditions are: firstly, heating to 100 ℃, and keeping the temperature for 2 hours; then heating to 150 ℃, and keeping the temperature for 4 hours; finally, the temperature is increased to 180 ℃, and the constant temperature is kept for 2 hours.
The invention has the beneficial effects that:
1. the invention grafts the voltage stabilizer on the silicon dioxide nano-particles by constructing a two-step liquid phase reaction to obtain m-ABA-SiO2Nanoparticles, after their incorporation in cycloaliphatic epoxy resins, due to SiO2The interface action of the nano particles and the alicyclic epoxy resin traps a part of charges, and meanwhile, the m-aminobenzoic acid captures a part of high-energy electrons, so that the charge distribution condition of a matrix under a certain voltage is improved, and the voltage breakdown resistance is improved.
2. The alicyclic epoxy resin nano composite insulating material has the advantages of good insulating property, good high-temperature resistance stability, large structural strength, good sealing property, no benzene ring, environmental protection and no toxicity to human bodies, and the decomposition product of the alicyclic epoxy resin nano composite insulating material is CO2And the gas micromolecules do not cause short circuit due to carbon formation, and the method has excellent application potential in the field of high-voltage insulation.
3. The invention has simple processing technology and easy operation, and can be cast into different shapes according to requirements.
Drawings
FIG. 1 shows a DSC curve (FIG. 1A) and an IR spectrum (FIG. 1B) of a cured cycloaliphatic epoxy resin under predetermined and optimal conditions.
FIG. 2 is a comparison graph of thermally stable TG of cured cycloaliphatic epoxy resin under preset and optimal conditions.
FIG. 3 is m-ABA-SiO2The synthesis mechanism of the nanoparticles is schematically shown.
FIG. 4 shows m-ABA-SiO2TEM image (fig. 4A) and ir spectrum (fig. 4B) of the nanoparticles.
FIG. 5 shows different m-ABA-SiO2SEM pictures of the obtained nano composite insulating material under the condition of the addition amount of the nano particles, wherein m-ABA-SiO correspond to the pictures (A) to (D) in sequence2The weight percentage of the nano particles is 0 wt%, 1 wt%, 3 wt% and 5 wt%.
FIG. 6 shows different m-ABA-SiO2TG curve of the obtained nano composite insulating material under the addition of the nano particles.
FIG. 7 shows different m-ABA-SiO2The thermal conductivity of the obtained nano composite insulating material under the condition of adding the nano particles.
FIG. 8 shows different m-ABA-SiO2The stress-strain curve of the obtained nano composite insulating material under the addition of the nano particles.
FIG. 9 shows different m-ABA-SiO2Volume resistivity of the resulting nanocomposite insulation material at the amount of nanoparticles added.
FIG. 10 shows different m-ABA-SiO2The voltage breakdown strength of the obtained nanocomposite insulation material with the addition of the nanoparticles, wherein: plot (A) shows the Weibull distribution of the breakdown strength of the nanocomposites, the solid line representing the fitting results using a two parameter Weibull distribution function; the histogram of FIG. B shows m-ABA-SiO in different mass percentages2Breakdown field strength of/CE.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. The following disclosure is merely exemplary and illustrative of the inventive concept, and those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Example 1
1. Determination of the curing Process
All glassware was ultrasonically cleaned with a magnetic stirrer and rinsed with ultra pure water prior to preparation.
Firstly, according to the properties of the curing agent, the proportion of the curing agent to the alicyclic epoxy resin (alicyclic epoxy resin: anhydride curing agent: 100: 80) and the curing process (100 ℃/2h +150 ℃/4h) are preset. Then adding liquid alicyclic epoxy resin and an anhydride curing agent into a beaker according to a preset proportioning condition, and fully stirring at room temperature to obtain a transparent solution; and curing the transparent solution according to preset curing conditions.
As shown in figure 1, a DSC curve (A) of the alicyclic epoxy resin cured under the preset condition has a curing exothermic peak between 150 and 250 ℃, and an infrared spectrogram (B) of 910cm-1The presence of epoxy groups indicates that the curing reaction did not proceed to completion. The proportion, curing time and temperature of the resin and the curing agent are regulated and controlled by a controlled variable method, the exothermic peak of curing is regulated and controlled by DSC until the exothermic peak disappears, and the optimal conditions obtained by regulation and control are as follows: the mass ratio of the liquid alicyclic epoxy resin, the anhydride curing agent and the accelerator DMP-30 is 100:120: 5; the curing conditions are 100 ℃/2h +150 ℃/4h +180 ℃/2h (firstly, the temperature is raised to 100 ℃, the temperature is kept for 2h, then, the temperature is raised to 150 ℃, the temperature is kept for 4h, and finally, the temperature is raised to 180 ℃, the temperature is kept for 2 h). The disappearance of the epoxy groups in the infrared spectrum of the cycloaliphatic epoxy resin after curing under the optimum curing conditions of fig. 1 also confirms that the cycloaliphatic epoxy resin system has been fully cured. Meanwhile, the thermal stability is also optimized after the curing conditions are optimized as can be seen from the thermally stable TG comparison curve of FIG. 2.
2. Preparation of m-ABA-SiO according to the scheme shown in FIG. 32Nanoparticles
2.21g of gamma-aminopropyltriethoxysilane (KH-550) and 1.37g of m-aminobenzoic acid (m-ABA) were weighed in a three-necked flask, 20mL of toluene was added, and stirring was carried out at 75 ℃ for 3 hours to obtain an amidated product.
20mL of toluene were added to the beaker, and 0.5g of gas phase SiO was added2And ultrasonically dispersing for 30min to obtain suspension.
Dripping the obtained suspension into amidation productAdding 2mL of distilled water after formation, stirring for 7h at 75 ℃, centrifuging, repeatedly cleaning the obtained product with ethanol, and drying to obtain m-ABA-SiO2And (3) nanoparticles.
FIG. 4 shows m-ABA-SiO2TEM image (fig. 4A) and ir spectrum (fig. 4B) of the nanoparticles. From the TEM image, m-ABA-SiO can be seen2The particle size of the nano particles is uniformly distributed around 20 nm. In the infrared spectrum, 2923cm-1In the presence of-CH2Peak of stretching vibration at 1395cm-1Has a stretching vibration peak of-C-N-at 1650cm-1A stretching vibration peak of 960cm at which-C ═ O-appears-1The bending vibration peak of Si-OH disappears, and the silicon dioxide is successfully grafted with the m-aminobenzoic acid.
3、m-ABA-SiO2Synthesis of alicyclic epoxy resin nano composite material insulation
Firstly, adding liquid alicyclic epoxy resin, an anhydride curing agent and an accelerator DMP-30 into a beaker according to the mass ratio of 100:120:5, and fully stirring at room temperature to obtain a light yellow transparent solution;
then adding m-ABA-SiO into the transparent solution under the condition of rapid stirring2Continuously stirring the nano particles until the solution is clarified again, and then ultrasonically crushing bubbles in the solution to obtain a mixed solution;
finally, curing the mixed solution (100 ℃/2h +150 ℃/4h +180 ℃/2h) to obtain the high-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material. For comparison of m-ABA-SiO2The influence of different addition amounts of the nano particles on the performance of the obtained nano composite insulating material, namely, m-ABA-SiO, four samples prepared in total in the embodiment2The nano particles respectively account for 0 wt%, 1 wt%, 3 wt% and 5 wt% of the mass of the nano composite insulating material.
FIG. 5 shows different m-ABA-SiO2SEM pictures of the obtained nano composite insulating material under the condition of adding the nano particles, wherein the pictures (A) to (D) correspond to m-ABA-SiO in sequence2The weight percentage of the nano particles is 0 wt%, 1 wt%, 3 wt% and 5 wt%. From FIG. 5, m-ABA-SiO can be seen2The nano composite insulating material with 5 wt% of nano particles dispersed in the matrixWith some aggregation and stacking of particles.
FIG. 6 shows different m-ABA-SiO2The TG curve of the resulting nanocomposite insulation with the amount of added nanoparticles can be seen as: the thermal decomposition temperature of the alicyclic epoxy matrix can reach 350 ℃, the introduced nano particles have little influence on the thermal stability of the alicyclic epoxy matrix, and the introduced nano particles slightly increase to about 355 ℃.
FIG. 7 shows different m-ABA-SiO2The thermal conductivity of the obtained nano composite insulating material under the addition of the nano particles can be seen to follow the thermal conductivity of m-ABA-SiO2The addition of the nanoparticles provides a certain improvement.
To characterize m-ABA-SiO2The tensile test was performed on the material by the change in tensile strength of the material after the nanoparticles were added, as shown in FIG. 8, m-ABA-SiO2The tensile strength of the matrix is improved by adding the epoxy resin, and the maximum tensile strength can reach 86.43MPa at 3 wt%, and is improved by 29.08% compared with a pure epoxy resin matrix.
As an insulating material, the volume resistivity of the material at room temperature was tested as shown in FIG. 9, with m-ABA-SiO2The volume resistivity is increased to a maximum of 5.47X 10 at 3 wt%14Omega.m, which is increased by 1.4 times compared with pure alicyclic epoxy resin.
In FIG. 10, m-ABA-SiO was obtained2Electrical breakdown performance of/CE nanocomposites. Where (A) measured the Weibull distribution of the breakdown strength of the nanocomposite and the solid line represents the fit using a two parameter Weibull distribution function. The histogram of the graph B visually represents m-ABA-SiO with different mass percentages2Impact on CE breakdown field strength. In m-ABA-SiO2When the content of the nano particles is less than 3 wt%, the change trend of the breakdown field intensity is increased along with the increase of the nano particles, the nano particles continue to increase, and the breakdown field intensity is reduced. In the process, the breakdown field strength reaches 53kV/mm at most. Compared with pure CE, the improvement is 40.8%.
From the comparison of the above properties, m-ABA-SiO2The introduction of nanoparticles is advantageous for improving the performance of pure cycloaliphatic epoxy resins.
The present invention is not limited to the above exemplary embodiments, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. High-voltage-resistant m-ABA-SiO2The alicyclic epoxy resin nano composite insulating material is characterized in that: the nano composite insulating material is prepared by adding SiO grafted with voltage stabilizer into alicyclic epoxy resin matrix2Nanoparticles, voltage stabilizer grafted SiO in said nanocomposite insulation material2The mass percentage of the nano particles is 1-5%;
the voltage stabilizer grafted SiO2The nanoparticles are in SiO2The nano particles are grafted with a voltage stabilizer m-aminobenzoic acid which is marked as m-ABA-SiO2A nanoparticle;
the m-ABA-SiO2The preparation method of the nano-particles comprises the following steps:
step 1, weighing 2.0-2.4g of gamma-aminopropyltriethoxysilane and 1.2-1.5g of m-aminobenzoic acid, placing in a three-neck flask, adding 20mL of toluene and 70-80 g of m-aminobenzoic acidoC, stirring for 3 hours to obtain an amidation product;
step 2, adding 20mL of toluene into a beaker, and then adding 0.4-0.6g of SiO2Ultrasonically dispersing uniformly to obtain a suspension;
step 3, dropwise adding the suspension obtained in the step 2 into the amidation product obtained in the step 1, and after the dropwise adding is finished, adding 2mL of distilled water and 70-80 percentoStirring for 6-8h under C, centrifuging, repeatedly cleaning the obtained product with ethanol, and drying to obtain m-ABA-SiO2And (3) nanoparticles.
2. High-voltage-resistant m-ABA-SiO film as claimed in claim 12The preparation method of the alicyclic epoxy resin nano composite insulating material is characterized by comprising the following steps:
firstly, adding liquid alicyclic epoxy resin, anhydride curing agent and accelerator DMP-30 into a beaker, and fully stirring at room temperature to obtain a transparent solution;
then m-ABA-SiO is added into the transparent solution under the condition of rapid stirring2Continuously stirring the nano particles until the solution is clear, and then performing ultrasonic dispersion uniformly to obtain a mixed solution;
finally, curing the mixed solution to obtain the high-voltage-resistant m-ABA-SiO2Alicyclic epoxy resin nano composite insulating material.
3. The method of claim 2, wherein: the mass ratio of the liquid alicyclic epoxy resin, the anhydride curing agent and the accelerator DMP-30 is 100:120: 5.
4. The method of claim 2, wherein: the curing conditions are as follows: first, the temperature is raised to 100 deg.CoC, keeping the temperature for 2 hours; then the temperature is raised to 150 DEGoC, keeping the temperature for 4 hours; finally heating to 180 DEGoAnd C, keeping the temperature for 2 hours.
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